并流滴加法制备大孔容纤维状γ-氧化铝

万艳春1 王玉军1 骆广生1

(1.化学工程联合国家重点实验室清华大学化学工程系, 北京 100084)

【摘要】以偏铝酸钠 (NaAlO2) -硫酸铝 (Al2 (SO4) 3) 为原料, 利用并流滴加法控制沉淀过程的反应pH, 并通过调节原料浓度、老化pH和加入表面活性剂十二烷基苯磺酸钠 (SDBS) 等方法, 成功制备得到了大孔容纤维状的γ-氧化铝。实验发现, 不同的原料浓度会影响成核-生长过程, 得到不规则片状、纤维状或颗粒状等不同形貌的γ-氧化铝, 其中纤维状可形成大孔容。当NaAlO2浓度为0.5~0.75 mol/L, 反应pH控制在8~9.5, 老化pH控制在9左右时, 得到的γ-氧化铝呈纤维状, 孔容较大;此外, 在老化过程中添加SDBS可进一步提高孔容, 并改善孔径分布。本方法成功制备出孔容为1.35~2.19 ml/g、比表面积为300~500 m2/g、平均孔径为14~21 nm的纤维状γ-氧化铝, 纤维长度为50~60 nm, 纤维宽度约5 nm, 可为渣油加氢过程提供一种性能良好的催化剂载体。

【关键词】 偏铝酸钠-硫酸铝; 沉淀法; γ-氧化铝; 并流滴加; 成核-生长; 表面活性剂;

【DOI】

【基金资助】 国家自然科学基金项目 (21276140, 21036002) 国家自然科学基金项目 (21276140, 21036002) 国家重点基础研究发展计划项目 (2013CB733600) 国家重点基础研究发展计划项目 (2013CB733600)

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    References

    [1]LI H Y, ZHANG T S, YANG N.The preparation and application of nanometer-Al2O3[J].Journal of Tianjin University of Light Industry, 2003, 18 (4) :34-37.

    [2]ZHOU K G, LI Y P, LI J C, et al.Preparation of fibrous nano-alumina by direct precipitation[J].Journal of Hunan University (Natural Sciences) , 2009, 36 (8) :59-63.

    [3]ZOU S, YANG Q, ZENG S, et al.The form of sulfate in pseudoboehmite and its effect on properties of pseudo-boehmite[J].China Petroleum Processing&Petrochemical Technology, 2014, 16 (4) :1-6.

    [4]CHEN W, YIN Z L, CHEN W, et al.Studying on alumina of catalyst substrate in automobile exhaust cleaning[J].New Technology&New Process, 2006, (2) :98-99.

    [5]WANG D C, LIU J D.Study on the hydrodemetallization catalyst using alumina support with build-up framework pore structure[J].Petroleum Processing and Petrochemicals, 2010, 41 (1) :31-35.

    [6]WANG C.The research on preparation method and loading catalytic performance of pyrolysis gasoline hydrogenation catalyst alumina supporter[D].Lanzhou:Lanzhou University of Technology, 2015.

    [7]ZENG S Q, YANG Q H, XIAO C W, et al.Effect of drying and aging conditions on the properties of pseudo-boehmite[J].Petroleum Processing and Petrochemicals, 2012, 43 (6) :53-57.

    [8]ZHANG L F, SHI Y, ZHAO B Y, et al.Progress in research onγ-alumina catalyst carrier[J].Materials Review, 2007, 21 (2) :67-71.

    [9]TONG J, LYU Z H, ZHANG X H.Study on synthesis of alumina with large pore volume and pore size[J].Contemporary Chemical Industry, 2016, 45 (6) :1104-1107.

    [10]RAO S M, ZHU J J, DU H R.Application and preparation of activated alumina with large pore volume[J].Light Metals, 2002, (3) :17-18.

    [11]DU M, SUN Z X.Recent development in the preparation of nanoalumina[J].Inorganic Chemicals Industry, 2005, 37 (12) :9-11.

    [12]THIRUCHITRAMBALAM M, PALKAR V R, GOPINATHAN V.Hydrolysis of aluminium metal and sol-gel processing of nano alumina[J].Materials Letters, 2004, 58 (24) :3063-3066.

    [13]DU S G, LIU Y.Preparation of seed crystals for superfine aluminum hydroxide powders by carbonization process[J].China Powder Science and Technology, 2011, 17 (4) :80-82.

    [14]WANG Y.Preparation of psedo-boehmite from sodium aluminate solution[J].Light Metals, 2010, (4) :19-20

    [15]YOLDAS B E.Transparent porous alumina[J].American Ceramic Society Bulletin, 1975, 54 (3) :286-288.

    [16]KOBAYASHI Y, ISHIZAKA T, KUROKAWA Y.Preparation of alumina films by the sol-gel method[J].Journal of Materials Science, 2005, 40 (2) :263-283.

    [17]ZHOU F, ZHANG Y, FAN H F.Researches on the preparation of pseudo-boemite with sodium aluminate-carbon dioxide process[J].World Nonferrous Metals, 2008, (5) :31-33.

    [18]CAO X Z, JIA C B.Discussion on the factors to impact dispersion index of pseudo boehmite[J].Energy Saving of Non-Ferrous Metallurgy, 2008, 24 (3) :30-33.

    [19]SHANG L D, WANG H H.Production and modification of activated alumina[J].Inorganic Chemicals Industry, 2012, 44 (1) :1-6.

    [20]WANG Y J, XU D Q, SUN H T, et al.Preparation of pseudoboehmite with a large pore volume and a large pore size by using a membranedispersion microstructured reactor through the reaction of CO2 and a Na Al O2 solution[J].Industrial&Engineering Chemistry Research, 2011, 50 (7) :3889-3894.

    [21]SUN Y, YE Y, JIN J.Preparation of nanosized alumina with low cost by precipitation method[J].Materials Review, 2007, 21 (S1) :150-152.

    [22]MENG W S.Study on preparation of nano-Al2O3 powder by precipitation methods[D].Wuhan:Wuhan University of Science and Technology, 2004.

    [23]YANG Y Y, JIANG S A, LI J J, et al.Influence of pH on crystal form of aluminum hydroxide[J].Inorganic Chemicals Industry, 2017, 49 (11) :41-43.

    [24]LIPPENS B C.Structure and texture of aluminas[D].USA:Waltman, 1961.

    [25]PENG L, XU X, LV Z, et al.Thermal and morphological study of Al2O3 nanofibers derived from boehmite precursor[J].Journal of Thermal Analysis and Calorimetry, 2012, 110 (2) :749-754.

    [26]LI S W, XU J H, LUO G S.The effect of oversaturation and mixing properties on crystal morphology[C]//2006 Annual Conference of Chinese Society of Particuology cum Symposium on Particle Technology across Taiwan Straits.Beijing:Chinese Society of Particuology, 2006:173-177.

    [27]MANTZARIS N V.Liquid-phase synthesis of nanoparticles:particle size distribution dynamics and control[J].Chemical Engineering Science, 2005, 60 (17) :4749-4770.

    [28]JUDAT B, RACINA A, KIND M.Macro-and micromixing in a TaylorCouette reactor with axial flow and their influence on the precipitation of barium sulfate[J].Chemical Engineering&Technology, 2004, 27 (3) :287-292.

    [30]LU S Y, HE Y Q.Application of surfactant to synthesis of nanoalumina[J].Materials Review, 2006, 20 (S1) :149-152.

    [30]SUN X J.Study on the application of surfactants in preparation and dispersion of ultra-fine alumina[J].Powder Metallurgy Technology, 2015, 33 (4) :254-258.

    [31]CAI W Q, LI H Q, ZHANG Y.Preparation of boehmites with novel morphologies via surfactants assisted hydrothermal synthesis[J].Materials Science and Technology, 2008, 16 (2) :207-210.

This Article

ISSN:0438-1157

CN: 11-1946/TQ

Vol 69, No. 11, Pages 4840-4847

November 2018

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Article Outline

摘要

  • 引言
  • 1 实验材料和方法
  • 2 实验结果与讨论
  • 3 结论
  • 符号说明
  • 参考文献